1
PROJECT REPORT
ON
EVALUATION OF SUITABILITY OF SUGARCANE WAX FOR APPLICATION
IN COSMETICS (Study I)
SUBMITTED TO
M/s GODAVARI BIOREFINERIES
MUMBAI
SUBMITTED BY
SHRIRAM INSTITUTE FOR INDUSTRIAL RESEARCH
19, UNIVERSITY ROAD, DELHI 110007
3
CONTENT
S. No. Particulars Page No.
1.0 Background 7
2.0 Scope of work (Study I) 8
3.0 Literature Survey 8
4.0 Work Carried Out 9
4.1 Lipstick 9
4.1.1 Identification of lipstick composition 9
4.1.2 Raw material specification 11
4.1.3 Methodology for preparation of lipstick composition 12
4.1.4 Designing and fabrication of mold for lipstick 13
4.1.5 Equipment used for the evaluation of lipstick salves 14
4.1.6 Characterization of Lipstick 17
4.1.7 Requirements of lipstick 19
4.2 Cosmetic pencil 20
4.2.1 Identification of composition for cosmetic pencil 20
4.2.2 Raw material specification 20
4.2.3 Methodology for preparation of cosmetic pencil
composition
22
4
4.2.4 Equipment used for the evaluation of cosmetic pencil 22
4.2.5 Characterization of cosmetic pencil 23
4.2.6 Requirements of cosmetic pencil 24
5.0 Results and discussion 24
5.1 Lipstick 24
5.2 Cosmetic pencil 25
6.0 Conclusion 26
REFERENCE 27
5
LIST OF TABLES
Table No. Particulars Page No.
1 Lipstick Composition (Reference: ‘Comprehensive
book on Cosmetics- Formulation, Manufacturing
and Quality control’ by. P. P. Sharma; Chapter-
16, pp 287-300, Vandana Publication, Delhi,
1998)
9
2 Lipstick Composition (Reference: US Patent
5093111, 1992)
10
3 Specification of raw materials used in lipstick
composition
11
4 Requirements of Lipstick 19
5 Composition for cosmetic pencil (Reference:
EP1048285A2, 2000)
20
6 Specification of raw materials used in cosmetic
pencil composition
21
7 Requirements of cosmetic pencil 24
8 Summary of results of lipstick 25
9 Summary of results of cosmetic pencil 26
6
LIST OF FIGURES
Figure No. Particulars Page No.
1a Lipstick mold holder 13
1b Lipstick molds with mold holder 14
1c Lipstick molds tapering dimensions (A) and front
dimension (B)
14
2 Softening point test apparatus for lipstick salve 15
3 Breaking load test apparatus for lipstick salve 16
4 Pay-off test apparatus for lipstick salve 17
5 Pay-off test apparatus for cosmetic pencil 23
7
1.0 Background
Sugarcane wax is attracting attention as a substitute of the natural
waxes. Sugarcane wax is found on the cane bark surface as a whitish to
dark yellow waxy substance. Its major function is the protection of bark
surface. The consumption of natural waxes like carnauba and candelila
waxes has increased in various application areas such as lubrication of
machinery, polishing of metallic surfaces, manufacture of cosmetics, food
ingredient, etc. As a result, their demand has also increased.
It is extracted from the press mud or filter cake mud, obtained after
sugarcane juice clarification, by solvent extraction technique. Sugarcane
wax is complex and variable mixture of long chain alkenes, hydrocarbons,
fatty acids, ketones, aldehydes, alcohols, esters, and steroids. Sugarcane
wax is indigestible and harmless to health. In its refined form it has a light
yellowish colour. Due to the high melting point of 75 to 80 °C sugarcane
wax remains stable even on exposure to direct sunlight.
The potential areas of sugarcane wax include pharmaceutical
preparations, confectionary items, processed food, carbon papers, carbon
less carbon papers, electrical insulations of cables and wires, paints &
varnishes, crayons, coloured pencils and cosmetics.
M/s Godavari Biorefineries, Mumbai is commercially producing sugarcane
wax under the trade name of “nautowax” and interested in its application
research in cosmetic and food industry. In order to explore potential use of
sugarcane wax in lipstick and cosmetic pencil formulations in place of
carnauba wax, the present project “evaluation of suitability of sugarcane
wax for application in cosmetics” was sanctioned.
Carnauba wax, also called Brazil wax or palm wax, is obtained from the
leaves of the carnauba palm. It is known as queen of waxes and in its
pure state, it usually comes in the form of hard yellow-brown flakes.
Because of its hypoallergenic and emollient properties as well as its shine,
8
carnauba wax appears as an ingredient in many cosmetic formulas where
it is used to thicken lipstick, eyeliner, mascara, eye shadow, foundation,
deodorant, various skin care preparations, sun care preparations, etc.
2.0 Scope of work (Study I)
¾ Procurement of cosmetic grade carnauba wax from market
¾ Procurement of sugarcane wax from M/s Godavari
¾ Identification and selection of standard formulations for lipstick and
cosmetic pencil
¾ Procurement of different ingredients to be used in formulation of
lipstick and cosmetic pencil
¾ Preparation of lipstick and cosmetic pencil formulations using
carnauba and sugarcane wax
¾ Modification of standard formulation to develop lipstick and
cosmetic pencil based on sugarcane wax to match its performance
equivalent to carnauba wax
¾ Comparative evaluation of lipstick and cosmetic pencil formulations
based on carnauba and sugarcane wax for various physico-
mechanical properties as per standard protocols (IS 9875: 1990 of
lipstick and IS 9832: 2002 of cosmetic pencil)
¾ Compilation of results and submission of report
3.0 Literature Survey
During the agro-industrial process, a large part of the wax gets dissolved
in the crude juice and gets separated as the waste during the subsequent
defecation-clarification step (filter cake from sugar refinery) or distillation [1-4].
Sugarcane wax is a potentially valuable by-product, extraction and
processing costs are relatively high, leaving a rather small profit margin [5-
7]. However, the new technologies can increase the viability of cane wax as
a byproduct from press mud [8].
9
Sugarcane wax recovery from filter cake/ press mud is well documented [9]
as are the relevant methods and techniques at the laboratory or industrial
level [10-12]. Sugarcane wax has always been a matter of interest, due to its
industrial applications, in particular in the cosmetic and pharmaceutical
industry [13-15]. It is a potential substitute for costly carnauba wax which is
widely used in cosmetics, food and pharmaceuticals. In addition,
sugarcane wax is also a source of long chain primary aliphatic alcohols,
which find applications as cholesterol-lowering products [16-18].
4.0 Work Carried Out
4.1 Lipstick
The work carried out on this project has been described in detail in this
section.
4.1.1 Identification of lipstick composition: For studying the feasibility
of using sugarcane wax in cosmetic formulations in place of carnauba
wax, various compositions have been identified from the literature as
presented in Tables 1-2.
Table-1: Lipstick Composition (Reference: ‘Comprehensive book on
Cosmetics- Formulation, Manufacturing and Quality control’ by. P. P.
Sharma; Chapter-16, pp 287-300, Vandana Publication, Delhi, 1998)
S. No. Ingredients Wt (%)
1 Castor oil 13
2 Isopropyl linolate 1.5
3 Isopropyl myristate 2.5
4 Beeswax 7
5 Lanolin 2
10
6 Ozokerite wax 6
7 Carnauba wax/sugarcane wax 5
8 Candelilla wax 8
9 Propylene glycol 4
10 Acetylated monoglyceride (solid) 6
11 Acetylated monoglyceride (liquid) 3
12 Propylene glycol mono-myristate 10
13 Bromo acids 2
14 Perfume, anti-oxidant & preservative q.s.
Table-2: Lipstick Composition (Reference: US Patent 5093111, 1992)
S. No. Ingredients Wt (%)
1 Castor oil 46.5
2 lanolin 3
3 Mineral oil 3
4 beeswax 3
5 Candelilla wax 5
6 Ceresin wax 5
7 Carnauba wax/sugarcane wax 2
11
8 Sorbitan sesquistearate 2
9 Colorants 10
10 Fragrance 0.35
11 Preservatives 0.15
4.1.2 Raw material specification
The raw materials required for the preparation of lipstick composition as
per the ingredients mentioned in Table-1 & 2 were procured. Their
specifications have been given in Table-3.
Table-3: Specification of raw materials used in lipstick composition
S.No. Material Specifications
B.P.
(ºC)
M.P
(ºC)
Sp.
Gravity
(g/cc)
Mol.
Wt.
Flash
point
(ºC)
1 Castor oil 313 -- 0.961 298 --
2 Lanolin 38 -- -- 756 237
3 Mineral oil 358 -- 0.8 -- --
4 Bees wax -- 63 0.958 415 204
5 Candelilla wax -- 70 0.985 -- --
6 Ceresin wax -- 74 0.916 -- 113
7 Carnauba wax -- 84 0.999 -- 299
8 Sugarcane wax -- 66 0.972 -- 290
12
9 Sorbitan
sesquistereate
359 -- -- 1061 162
10 Isopropyl linoleate 179 -- 0.87 322 191
11 Isopropyl myristate 167 -- 0.85 270 --
12 Ozokerite wax -- 74 0.92 -- --
13 Propylene glycol 188 1.036 76
14 Acetylated
monoglyceride
-- -- 0.96-1.1 1742 --
15 Propylene glycol
mono-myristate
392 -- -- 286 300
16 Bromo acid (D&C
Red No. 21)
-- 295 -- 648 --
4.1.3 Methodology for preparation of lipstick composition
Firstly, the formulation mentioned in Table-1 was prepared. The lipstick
salve prepared by following the formulation given in Table-1 was not
comprable with the commercial product. Then, the formulation mentioned
in Table-2 was prepared and its apperance was found to be comprable
with the commercial lipstick sasmple. Hence, out of the two formulations
identified, the formulation given in Table-2 (USP 5093111, 1992) was
selected for study.
The lipstick composition was prepared by melt mixing of all the
components as mentioned in Table-2. Firstly, the liquid components
(castor oil, mineral oil and lanolin) were mixed and heated in a water bath
at 90-100 ºC. To this, the chosen colorant Bromo acid (D&C Red No. 21)
13
was added after sieving through 38 micron size (Amil Ltd.) to get a
homogenous mixture. The waxes were added to this homogenous mixture
and melt mixed at 90-100 ºC. While adding the waxes mentioned in the
composition given in Table-2, either carnauba wax was used or in its place
sugarcane wax was added. In the homogeneous composition prepared
after wax addition, sorbitan sesquistereate was added.
The molten mass was poured in to lipstick mold and then cooled to
ambient temperature. The lipstick salve was then removed from the mold
and stored for further use.
4.1.4 Designing and fabrication of mold for lipstick
For the development of lipstick salve, a mold was designed in SS-304
having length 52 mm, outer diameter 25 mm and inner diameter 14 mm
with one end having tapered dimension to give shape to lipstick. A mold
holder was also designed as shown in Figure-1 (a-c).
Figure-1a: Lipstick mold holder
14
Figure-1b: Lipstick molds with mold holder
Figure-1c: Lipstick molds tapering dimensions (A) and front dimension (B)
4.1.5 Equipment used for the evaluation of lipstick salves
The characterization of developed lipstick slaves based on carnauba and
sugarcane wax and the commercial lipstick sample (Lakme) was carried
out as per IS 9875, 1990 (reaffirmed 2005).
a) Softening point test apparatus: The apparatus comprises of a
controlled temperature water bath, a 12 cm long flat bottom tube
having diameter 2.5 cm and 0.1°C accurate thermometer (Figure-2).
A B
15
Figure-2: Softening point test apparatus for lipstick salve
b) Braking load test apparatus: This equipment measures the maximum
load which a lipstick can withstand before it breaks. It comprises of a
burette of 500 ml capacity held in screw chuck and an aluminum cup
of 6 cm diameter and 12 cm length with an arrangement of a hook to
suspend it on lipstick salve (Figure-3).
16
Figure-3: Breaking load test apparatus for lipstick salve
c) Pay off test apparatus: It helps in evaluating the mass release from the
lipstick salve. It consists of a constant speed electric motor of power
180 watt (0.25 hp approximately) attached to a gear arrangement,
which pulls the strip of paper (about 7 cm wide) from one roller on to
another roller fixed on platform through supports. A slot arrangement
having a cylindrical tube of 5.5 cm length and 2.2 cm diameter is also
fixed on the platform for holding the lipstick sample (Figure-4)
perpendicular to the tip of paper.
17
Figure-4: Pay-off test apparatus for lipstick salve
4.1.6 Characterization of Lipstick
Lipstick compositions prepared were evaluated for various properties as
per IS 9875, 1990 (reaffirmed 2005).
Softening point: Lipstick was placed with protruded salve in the flat
bottom tube and a thermometer was fixed through a cork in such a way
that the bulb of the thermometer just touched the lipstick salve. This
arrangement was placed in a 1-litre beaker filled with water such that
water level was 1 cm above the upper tip of the lipstick salve and the
beaker was placed in a water bath (Figure-2). Water was heated slowly
while stirring so that temperature rises at a rate of 2°C per minute. When
the temperature reached about 45°C, the rate of heating was decreased to
1°C per minute. The lipstick salve was observed constantly and the
temperature at which the salve starts bending and losing its shape was
recorded as its softening point.
Breaking load: The breaking load of the lipstick salve is the measure of its
firmness and strength. The lipstick container was fixed firmly with
18
protruded salve of diameter ranging 11 to 13 mm, into a screw type of
chuck so that the assembly was perfectly horizontal. The burette was
adjusted just above the lipstick salve and a marking was made at a
distance of 1.5 cm from the base of the salve where lipstick salve sited in
salve holder cup (Figure-3). Weight of aluminium container was taken
along with hook and suspended it on this 1.5 cm mark. Water was slowly
released from the burette into the aluminium container till the salve was
broken. Burette reading added with the mass of the suspended container
gives the breaking load of the lipstick.
Pay off test: 1 cm portion of lipstick salve was chopped off from the tip
using a sharp blade and the remaining portion of the salve was rubbed on
a piece of paper to make the end portion perfectly flat. The constant speed
motor was run and the time required for pulling out 100 cm of paper
length was determined. The preweighed lipstick salve having flat end was
inserted in the slot arrangement provided in pay off apparatus such that
the flattened salve portion rested on the surface of the paper strip (Figure-
4). A total load of 53 g was placed including mass of the 1ipstick.
Constant speed motor was started and with the help of stopwatch, 120 cm
length of paper was allowed to run. The lipstick salve was reweighed after
the rub off and the length and width of the line drawn on the paper strip
was measured. The pay off value was calculated using formula:
Pay-off (g/cm2) = (M1-M2)
l x b
Where, Ml is the mass in gram of the lipstick before the test; M2 is the
mass in gram of the lipstick after the test; l is the length in cm of the line
drawn on paper strip and b is breadth in cm of the line drawn on paper
strip.
19
4.1.7 Requirements of lipstick
Requirements for the lipstick salve as per IS specification are given in
Table-4.
Table-4: Requirements of Lipstick
S.No. Test Requirement Reference
1 Softening point, Min 55 ºC
IS 9875: 1990 2 Breaking load value, Min 200 g
3 Pay off test, Min 0.0001 g/cm2
20
4.2 Cosmetic pencil
4.2.1 Identification of composition for cosmetic pencil: In order to
study the suitability of sugarcane wax in cosmetic pencil in place of
carnauba wax, the composition mentioned in table-5 was identified from
the literature for the development of cosmetic pencil.
Table-5: Composition for cosmetic pencil (Reference: EP1048285A2, 2000)
S.No. Ingredients Wt (%)
1 Ceresin wax 12.35
2 Bees wax 1.15
3 Carnauba / sugarcane wax 8.5
4 Propyl paraben 0.1
5 Lanolin (anhydrous) 11.5
6 Isopropyl myristate 10.0
7 Talc 8.0
8 Iron oxide (black) 3.0
4.2.2 Raw material specification
The raw materials required for the preparation of cosmetic pencil
composition as per the ingredients mentioned in Table-5 were procured.
Their specifications have been given in Table-6.
21
Table-6: Specification of raw materials used in cosmetic pencil
composition
S.No. Material Specifications
B.P.
(ºC)
M.P
(ºC)
Sp. Gravity
(g/cc)
Mol.
Wt.
Flash point
(ºC)
1 Ceresin wax -- 74 0.916 -- 113
2 Bees wax -- 63 0.958 415 204.4
3 Carnauba
wax
-- 84 0.999 -- 299
4 Sugarcane
wax
-- 66 0.972 -- 290
5 Propyl
paraben
-- 96 1.06 180 --
6 Isopropyl
myristate
167 -- 0.85 270 --
7 Lanolin 38 -- -- 756 237
8 Talc -- 800 2.7 -- --
9 Iron oxide
(black)
-- >1000 1.5 -- --
22
4.2.3 Methodology for preparation of cosmetic pencil composition
The composition for cosmetic pencil was made by melt mixing of all the
components as mentioned in Table-5. Firstly, the liquid portions (castor
oil, lanolin and isopropyl myristate) were heated in a water bath at 90-100
ºC, and to this the chosen colorant Iron oxide (black) was added to get
homogenous mixture. The waxes were added to this homogenous mixture
and melt mixed. Lastly, propyl paraben was added in to this homogenous
mixture.
Molten mass was poured in a hollow tube of 3-4 mm diameter, cooled to
ambient temperature. The cosmetic pencil was then removed from the
mold and stored for further use.
4.2.4 Equipment used for the evaluation of cosmetic pencil
The characterization of developed cosmetic pencil based on carnauba and
sugarcane wax and the commercial cosmetic pencil (Lakme) was carried
out as per IS 9832, 2000.
Pay off test apparatus helps in evaluating the mass release from the
cosmetic pencil. It consists of a constant speed electric motor of power 180
watt (0.25 hp) attached to gear arrangement, which pulls the strip of
paper (about 7 cm wide) from one roller on to another roller fixed on a
platform through supports. A slot arrangement having a cylindrical tube
of 5.5 cm length and 1 cm diameter (inner) was fixed on the platform for
holding the cosmetic pencil sample perpendicular to the paper sheet
(Figure-5).
23
Figure 5: Pay-off test apparatus for cosmetic pencil
4.2.5 Characterization of cosmetic pencil
Cosmetic pencil compositions prepared were evaluated for pay off property
as per IS 9832, 2000.
Pay off test: Cosmetic pencil tip was held on the paper strip kept on the
machine in vertical position by a holder attached to the instrument. A load
of 80.5 g was placed on the other end of the pencil. Machine was started
so that the paper strip is pulled at a speed of about 5 cm/s. By doing this,
a line was drawn on the paper by wearing out the pencil slip for exactly
100 cm. The cosmetic pencil was reweighed after the rub off and the
length and width of the line drawn on the paper strip was measured. The
pay-off was determined by finding out the wear of slip in mg/100 cm2 area
of line drawn on strip of papers.
Pay-off (mg/100 cm2) = (M1-M2) x 1000 x 100
A x B
24
Where, Ml is the mass in grams of the slip before the test; M2 is the mass
in grams of the slip after the test; A is the diameter of slip in cm and B is
the length of paper in cm on which the pay off test is carried.
4.2.6 Requirements of cosmetic pencil
Requirement for the cosmetic pencil as per IS specification is given in
Table-7.
Table 7: Requirements of cosmetic pencil
S.No. Test Requirement Reference
1 Pay off 2 mg/100 cm2 (Min.) IS 9832: 2002
5.0 Results and discussion
5.1 Lipstick
The lipstick composition prepared using carnauba wax and sugarcane
wax were evaluated for softening point, breaking load and pay off. The
commercial sample of lipstick of Lakme brand was also evaluated for these
properties.
All the results were reported as an average of five samples for all
mentioned properties. The results for softening point, breaking load and
pay off test for commercial sample (Lakme), carnauba wax and sugarcane
wax have been summarized in Table-8.
As evident from the results, softening points of all three lipstick samples
i.e. commercial sample and the compositions made at SRI using carnauba
wax and sugarcane wax were more than 55 ºC, which is the minimum
requirement as per IS 9875, 1990. Hence, all three samples of lipsticks
are passing the test for softening point.
25
The breaking load values for all samples were found to be less than 200g,
which is the requirement as per IS 9875, 1990. The values for SRI
developed samples are much close to the required value of 200g as
compared to the commercial samples.
The pay off values for all three lipstick samples was more than 0.0001
g/cm2, which is the minimum requirement. Hence, all three samples of
lipsticks were passing the pay off test.
Table-8: Summary of results of lipstick
Property Requirement
(Minimum) Commercial
sample
(Lakme)
SRI developed using
Carnauba
wax
Sugarcane
wax
Softening point
(ºC)
55 61.8 63.3 61.2
Breaking load
(g)
200 107 193 192
Pay off (g/cm2) 0.0001 0.00058 0.00065 0.00051
5.2 Cosmetic pencil
The cosmetic pencil composition prepared using carnauba wax and
sugarcane wax were evaluated for pay off test. The commercial sample of
cosmetic pencil of Lakme brand was also evaluated for the same property.
The results reported are an average of five samples tested for the
mentioned property. The results for pay off test for commercial sample
(Lakme), carnauba wax and sugarcane wax have been summarized in
Table-9.
26
Table 9: Summary of results of cosmetic pencil
Property Requirement Commercial
sample
(Lakme)
SRI developed using
Carnauba
wax
Sugarcane
wax
Pay off
(mg/100 cm2)
2 (Min.) 2.08 2.24 2.38
As evident from the results, it was observed that the pay off tests for all
three cosmetic pencil samples i.e. commercial sample and the composition
made at SRI using carnauba wax and sugarcane wax were more than 2
mg/100 cm2, which is the minimum requirement as per IS 9832, 2002.
Hence, all three samples of cosmetic pencils were passing the pay off test.
6.0 Conclusion
¾ The preparation of lipstick and cosmetic pencil compositions has
been carried out successfully by replacing carnauba wax with
sugarcane wax in the compositions.
¾ The property profile of lipstick and cosmetic pencil compositions
prepared using sugarcane wax conformed with the requirements
specified in IS 9875: 1990 of lipstick and IS 9832: 2002 of cosmetic
pencil specifications.
¾ Property profile of lipstick and cosmetic pencil prepared using
carnauba wax and sugarcane wax was found to be comparable and
meeting the requirements given in IS 9875: 1990 of lipstick and IS
9832: 2002 of cosmetic pencil except for breaking load of lipstick.
27
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